Modification of HPTLC-plates by in situ chemical bonding with non-polar and polar organosilanes

A method has been developed for the preparation of modified silica plates for high performance thin-layer chromatography (HPTLC). Some typical organosilanes were thus allowed to react in situ with the silica of Merck HPTLC-plates. This method was found to be highly reproducible, simple and cheap. Non-polar plates were prepared and compared with commercial plates from Merck, Whatman and Macherey-Nagel. Modification with cyanodecyltrichlorosilane resulted in plates that showed good coverage, efficiency and low residual silica activity. Silica modified with a multifunctional silane has different properties in different organic solvents. It will appear to be non-polar in a polar solvent and vice versa. New advantageous separation systems are thus made feasible by the presence of cyano groups on the plate. The utility of modified thin-layer plates is demonstrated by the separation of some homologues of p-hydroxybenzoic acid esters and of some polycyclic aromatic hydrocarbons.     

Full Non-rigid Group of Sponge and Pina

The non-rigid molecule group theory (NRG) in which the dynamical symmetry operations are defined as physical operations is a new field in chemistry. Smeyers and Villa computed the r-NRG of the triple equivalent methyl rotation in pyramidal trimethylamine with inversion and proved that the r-NRG of this molecule is a group of order 648, containing a subgroup of order 324 without inversions (see J. Math. Chem. 28(4) (2000) 377–388). In this work, a computational method is described, by means of which it is possible to calculate the symmetry group of molecules. We study the full non-rigid group (f-NRG) of Sponge and Pina molecules with C ₂ and C _i point groups, respectively. It proved that these are groups of order 162 and 13122 with 54 and 3240 conjugacy classes, respectively. The character tables of these groups are also computed.     

Electron transfer from dibenzo[b,f]-1-azapentalene dianion: Attempted synthesis of dibenzo[b,f]-1-azapentalene

When dibenzo[b,f]-1-azapentalene dianion (3) was allowed to react with either iron (III) chloride or ethylene bromide, a one-electron transfer from3 took place readily to give the radical anion11. Further electron transfer from11 did not occur presumably due to the antiaromatic character of dibenzo[b,f]-1-azapentalene (1) that would have resulted. The radical anion11 underwent further transformation by hydrogen abstraction from the solvent to give 5,10-dihydroindeno[1,2-b]indole (2) and by dimerization to themeso and (R,S) isomers of 5,5,10,10-tetrahydro-10,10-biindeno[1,2-b]indole (4 a and4 b) respectively.

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Elektronentransfer von Dibenzo[b,f]-1-azapentalen-Dianion: Ein Versuch zur Synthese von Dibenzo[b,f]-1-azapentalen

Zusammenfassung Die Reaktion von Dibenzo[b,f]-1-azapentalen-Dianion (3) mit Eisen (III) oder Ethylenbromid ergab einen Ein-Elektronentransfer zum Radikalanion11. Ein weiterer Elektronentransfer fand nicht statt, vermutlich wegen des antiaromatischen Charakters von Dibenzo[b,f]-1-azapentalen (1), das dabei entstehen müßte. Das Radikalanion11 ergab unter Wasserstoffentzug aus dem Lösungsmittel 5,10-Dihydroindeno[1,2-b]indol (2), das weiter zummeso- bzw. (R,S)-5,5,10,10-tetrahydro-10,10-biindeno[1,2-b]indol (4 a bzw.4 b) dimerisierte.

     

CuO超细粉体的形貌与红外特性研究

CuO作为一种多功能精细无机材料，在印染、陶瓷、玻璃及医药等领域的应用已有数十年的历史，作为催化剂的主要活性成分，近年来在氧化、加氢、C１化学合成、NOx还原、CO及碳氢化合物燃烧、精细化工等多种催化反应中也得到了广泛的应用。可以推测，当CuO材料的粒度达到纳米级时，将使它的功能更加独特，应用更为广泛。因此CuO纳米材料的制备方法、聚集状态、与其他组分或载体的作用状况及催化活性等成为当前功能材料发展的研究热点之一犤１～８犦。我们在前文中报道了直接热解Cu２（OH）２CO３所得CuO粒径小、分布均匀、比表面积大，…     

Thermodynamics of Binary and Ternary Copper-, Cadmium,and Indium-Containing Semiconducting Phases: An Electrochemical Study

Optimum compositions of ion-selective membranes in quasi-binary systems CuCl-CdCl₂, LiCl-CdCl₂, and In₂S₃-InCl₃ are selected by a method of coulometric titration in cells with solid electrolytes. Transport numbers for ions are close to unity for the optimum compositions; transport numbers for electrons are vanishingly small ( ≺10⁻³ to 10⁻⁴); the electroconductivity is equal to ≈ 10⁻³ S cm⁻¹ at 200°C; the diffusion coefficients for the current-producing component are on the order of 10⁻⁶ to 10⁻⁷ cm² s⁻¹. When using a solid electrolyte of the composition CuCl-CdCl₂, which contains 30 mol % CdCl₂, methods of emf and electroconduction reveal that the region of homogeneity of copper(I) selenide falls in the region of compositions Cu_1.33Se-Cu_2.67Se.__________Translated from Elektrokhimiya, Vol. 41, No. 6, 2005, pp. 721–727.Original Russian Text Copyright © 2005 by Leushina, Kolesnikova, Makhanova, Zlomanov.Published on the basis of a report delivered at the VII Meeting on Fundamental Problems in Solid-State Ionics (Chernogolovka-2004).     

Darstellung, 11B-NMR-, Schwingungsspektren und Kristallstruktur von [(C5H5N)2CH2][1-(O2N)B10H9]

Preparation, ¹¹B NMR, Vibrational Spectra, and Crystal Structure of [(C₅H₅N)₂CH₂][1-(O₂N)B₁₀H₉] By reaction of [B₁₀H₁₀]^2? in aqueous acetonitrile with a saturated solution of NO₂ in dichloromethane [1-(O₂N) · B₁₀H₉]^2? and [B₁₀H₉(NO)B₁₀H₉]^3? are formed which can be separated by ion exchange chromatography on diethylaminoethyl(DEAE) cellulose from the starting compound. The X-ray structure determination of [(C₅H₅N)₂CH₂][1-(O₂N)B₁₀H₉] (triclinic, space group P1 , a = 7.1530(9), b = 8.3753(8), c = 15.198(2) Å, α = 96.00(1), β = 95.48(1), γ = 95.60(1)°, Z = 2) reveals the coordination of the NO₂ group via N with a B1? N distance of 1.535(5) Å and an O2? N? O1 angle of 119.3(3)°. The ¹¹B NMR spectrum exhibits the characteristic feature (1 : 1 : 4 : 4) of an apical monosubstituted B₁₀ cluster with a strong downfield shift of the ipso-B atom at +13.4 ppm. The IR and Raman spectra show strong NO stretching vibrations at 1381 und 1420 cm^?1.     

新型聚醚的合成与表征

用高活性催化剂催化环氧丙烷开环聚合得到一类新型高质量聚醚。对产物进行IR和NMR表征和分析,并探讨了合成工艺条件。结果表明,调节单体与调节剂的比例,控制反应温度在100 5℃,压力在0.15 ~ 0.25 MPa ,可得到不饱和度低、相对分子质量可控、相对分子质量分布窄的聚醚产品。     

混凝土中的声发射波速特性及其在源定位中的应用

利用声发射技术监测受载混凝土裂缝发展特征的首要任务是对声发射源的准确定位.为了解混凝土中声发射波速特性,提高声发射源定位精度,该文开展了一系列室内试验,构建了考虑衰减现象的声发射波速修正模型,优化建立了基于修正波速的区域穷举定位法.结果表明:水灰比越小,基准波速越大,波速随距离的衰减越大.骨料粒径越大,基准波速越大,波...     

应用不同光谱技术,动物RBC,Hb及人皮肤表面血流氧化-还原状态检测

目的:检测与分析实验动物血液RBC(RBC·O2,RBC·CO2),Hb(HbO2,HbCO2)和人体皮肤表面流动血液氧化·还原状态的成像与未成像可见光谱领域OD值特征,并为该技术对白癜风病表皮黑色素颗粒检测中的应用尊定基础。方法:利用不同光谱技术和invitro和invivo检测手段,统计分析血液不同状态下波长与位置的OD值信息。结果:invitro检测:动物血液Hb·O2和RBC·O2两者在可见领域均有367,414(Soret带)nm与541,576(Q带)nm的吸收峰位;血液Hb·CO2和RBC·CO2均有432(Soret带)与和553(Q带)nm的波长吸收峰位;血液RBC状态和Hb溶血状态波长吸收峰位无改变,只是在氧化与还原状态下有完全独立的吸收峰位,血液RBC状态和Hb溶血状态波长吸光度OD值之间,有显著性差异(p<0·01)。浓度为1·5×107cell·mL-1的RBC·O2和Hb·O2在576nm的吸收峰位吸光度(y)与红细胞浓度(x)做成两条回归曲线:既,Hb·O2(b1)^y=0·05 0·983x;RBC·O2(b2)y^=0·127 1·934x,两者之间差异有显著性(p<0·01)。invivo检测:在人手背皮肤表面ImSpector图像中RBC·O2状态在540,576nm,RBC·CO2状态在555和755nm处有吸收峰。选择(a:指甲,b:指,c:手背)三个点位分别进行波长检测,每点(n=10)545nm吸收峰的平均OD值,依次为0·83±0·001,0·73±0·001和0·62±0·001,其三处测定点的OD值之间有显著性差异(p<0·01)。结论:invitro检测的RBC与Hb两者波长吸收峰位不变,但吸光度OD值不同,认为RBC状态测定结果更接近于活体组织血管内原始状态。invivo检测对人体无任何侵袭与损伤,灵敏度高,测试时间短,并且同时获得被测样品的波长与位置信息画面等优势,有望表皮中黑素等有色颗粒的直接检测。     

双酚A人工抗原的光谱表征及免疫鉴定研究

双酚A(bisphenol A,BPA)是一种酚类环境雌激素,即使极低剂量残留对人类健康也有危害。为了建立其简单快速并适应现场检测的免疫分析方法,必须先合成它的人工抗原并进行鉴定。通过对双酚A进行结构修饰,用碳二亚胺将结构修饰了的双酚A与牛血清蛋白相偶联,经透析得到纯的双酚A人工抗原并冷冻干燥备用。然后用紫外光谱、红外光谱和免疫方法对人工抗原进行鉴定。结果表明,合成的人工抗原紫外光谱图中具有蛋白质和双酚A的特征吸收峰;人工抗原红外光谱图中呈现双酚A和牛血清蛋白的红外特征吸收峰;通过竞争ELISA试验表明用合成的人工抗原免疫的Balb/c小鼠血清中产生了双酚A的抗体。三种方法综合鉴定结果表明双酚A人工抗原合成成功,该人工抗原可以进一步用于制备抗双酚A的单克隆抗体。